CN110201557B - Large-flux reinforced ultrafiltration membrane and preparation method thereof - Google Patents
Large-flux reinforced ultrafiltration membrane and preparation method thereof Download PDFInfo
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- CN110201557B CN110201557B CN201910482575.4A CN201910482575A CN110201557B CN 110201557 B CN110201557 B CN 110201557B CN 201910482575 A CN201910482575 A CN 201910482575A CN 110201557 B CN110201557 B CN 110201557B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
Abstract
The invention relates to a large-flux reinforced ultrafiltration membrane which is composed of the following components in parts by weight: 30-40 parts of dopamine modified polyvinyl chloride; 10-20 parts of a hydrophilic agent; 40-50 parts of a polar solvent; 10-20 parts of a pore-foaming agent; and 5-15 parts of an auxiliary agent. According to the invention, the hydrophilic agent, the auxiliary agent and the dopamine modified polyvinyl chloride are blended and modified in a polar solvent, so that the surface tension of the membrane surface and the surface tension of the inner wall of a membrane hole are reduced, the hydrophilicity of the polyvinyl chloride is improved, and the triethanolamine in the hydrophilic agent, the polar bond in the auxiliary agent and the polar bond in the dopamine composite layer generate hydrogen bond interaction and attract each other, so that the hydrophilicity can be maintained for a long time, the anti-pollution performance of the ultrafiltration membrane is improved, and higher operation flux is kept for a long time; in addition, the small molecular pore-forming agent is not easy to block pores, has good film forming performance and good pure water flux, has low entanglement degree with the main material and is easy to separate from the surface of the membrane; the auxiliary agent effectively improves the melt processability and greatly enhances the mechanical property.
Description
Technical Field
The invention relates to the technical field of ultrafiltration membranes, in particular to a large-flux reinforced ultrafiltration membrane and a preparation method thereof.
Background
The ultrafiltration is a membrane separation process which uses pressure difference as a driving force, utilizes a screening mechanism to intercept macromolecular solutes according to different sizes of substances, and realizes separation with solvents or micromolecular solutes, and the effective pore diameter of the used ultrafiltration membrane is 2-100 nm. The method can realize separation and purification of substances with different molecular weights by utilizing the screening effect of micropores on the surface of the ultrafiltration membrane, has a good effect on removing particles, colloids, bacteria and various organic matters, and is widely applied to related fields of water treatment, food, electronics, machinery, chemical industry, petroleum, environmental protection, medicine, biotechnology and the like in recent years.
Currently, ultrafiltration membranes are mainly made of high molecular materials, and are the main materials of ultrafiltration membranes due to the advantages of multiple types, controllable chemical composition and structure, low price, good film forming property and the like, and account for more than 90% of the total membrane materials. The commercial polymer membrane materials mainly comprise cellulose acetate, cellulose nitrate, regenerated cellulose, polypropylene, polytetrafluoroethylene, polyvinylidene fluoride, polyvinyl chloride, polysulfone, polyarylethersulfone, polymethyl carbonate and the like. The ultrafiltration membrane in the prior art has poor hydrophilicity, is easy to adsorb pollutants in the using process, reduces the treatment efficiency and the like, and needs to be further improved.
Disclosure of Invention
In order to overcome the technical defects in the prior art, the invention provides a large-flux reinforced ultrafiltration membrane and a preparation method thereof.
The technical solution adopted by the invention is as follows:
a large-flux reinforced ultrafiltration membrane comprises the following components in parts by weight: 30-40 parts of dopamine modified polyvinyl chloride; 10-20 parts of a hydrophilic agent; 40-50 parts of a polar solvent; 10-20 parts of a pore-foaming agent; and 5-15 parts of an auxiliary agent.
Preferably, the polar solvent is dimethylformamide or dimethylacetamide.
Preferably, the pore-forming agent is one or more of hypromellose, talcum powder, wood powder, polyethylene glycol 300 and polyethylene glycol 600.
Preferably, the hydrophilic agent comprises 50-100% by mass of triethanolamine.
Preferably, the hydrophilic agent further comprises one or more of polyethylene glycol, polysorbate, cellulose acetate, propylene oxide-epoxy hexane copolymer, triethanolamine oleate, dioctyl sodium sulfosuccinate, sodium lauryl sulfate, and sodium cetyl alcohol sulfate.
Preferably, the auxiliary agent is one or more of polymethyl methacrylate, polysulfone, polypropylene, polyethylene, polystyrene, dibutyl phthalate, diisodecyl phthalate and dioctyl phthalate.
The invention also provides a preparation method of the large-flux reinforced ultrafiltration membrane, which comprises the following steps:
s1, adding the dopamine modified polyvinyl chloride, the solvent, the hydrophilic agent, the pore-forming agent and the auxiliary agent into a stirring kettle respectively according to the proportion, stirring and mixing for 24 hours, controlling the temperature at 90-95 ℃ and the stirring speed at 100HZ, and obtaining a casting solution;
s2, conveying the stirred casting film liquid to a reaction kettle through a conveying pump for vacuum foaming for 12 hours;
s3, after defoaming, inputting the casting solution into a spinneret plate of a spinning machine through a metering pump, mixing the casting solution with pure water core solution, and then feeding the mixture into a coagulating bath for reaction, wherein the surface of the casting solution and the surface of the hollow fiber are coagulated and occluded after entering the water surface of the coagulating bath to generate a core liquid film;
s4, stretching the core liquid film through a wire winding wheel and bringing the core liquid film into a washing tank for collection and cutting;
s5, after the collection is finished, the core liquid film is immersed in 10-50% glycerol aqueous solution for 5-8 h and then dried.
Wherein: the preparation method of the dopamine modified polyvinyl chloride specifically comprises the following steps:
s1.1, dissolving Tris (hydroxymethyl) aminomethane in distilled water, and adjusting the pH to 8.5 by using hydrochloric acid to obtain a Tris-HCl buffer solution;
s1.2, rapidly adding polyvinyl chloride powder and ethanol or isopropanol or glycerol into the Tris-HCl buffer solution obtained in the step 1.1 under the condition of continuously magnetically stirring at room temperature;
s1.3, magnetically stirring the mixed solution obtained in the step S1.2 at 25 ℃ for 6-24 hours;
s1.4, carrying out suction filtration on the product obtained in the step S1.3, then washing with deionized water, centrifuging for 3 times, and placing the obtained product in a vacuum drier at 40 ℃ to dry to constant weight to obtain the dopamine modified polyvinyl chloride.
The invention has the beneficial effects that:
the invention adopts hydrophilic agent, auxiliary agent and dopamine modified polyvinyl chloride to be blended and modified in polar solvent, reduces the surface tension of the membrane surface and the inner wall of the membrane pore, improves the hydrophilicity of the polyvinyl chloride, simultaneously, the dopamine in the dopamine modified polyvinyl chloride contains catechol group and amino group, easily generates self-polymerization reaction under the oxidation action of dissolved oxygen to form a firmly attached dopamine composite layer on the polyvinyl chloride surface, the acting force is between covalent bond and non-covalent bond, and has stronger stability and durability, then, the hydrophilic agent contains triethanolamine, the triethanolamine not only contains abundant hydroxyl hydrophilic group, but also the nitrogen atom has strong electronegativity, has stronger lone electron pair, and can be combined with the polar bond in the auxiliary agent and the dopaminePolar bonds in the composite layer generate hydrogen bonds to attract each other, so that the problem of hydrophilic performance reduction caused by loss of hydrophilic additives in the ultrafiltration membrane after use can be solved, the hydrophilicity can be maintained for a long time, the pollution resistance of the ultrafiltration membrane is improved, the higher running flux is durably kept, and the pure water flux is 400-600L/M (liter/mass)/M at the pressure of 0.1MPa and the temperature of 25 DEG C2H, the filtration precision reaches 0.01 micron; in addition, the triethanolamine can perform coordination reaction with calcium, magnesium, iron and other ions, and has good removal effect on metal ions in the sewage.
In addition, the small molecular pore-forming agent is not easy to block pores, has good film forming performance and good pure water flux, has low entanglement degree with the main material and is easy to separate from the surface of the membrane; the auxiliary agent effectively improves the melt processability, greatly enhances the mechanical property, has high reaction temperature and enhances the tensile strength and the elongation at break.
Detailed Description
Example 1
The embodiment provides a large-flux reinforced ultrafiltration membrane which is composed of the following components in parts by weight: 30 parts of dopamine modified polyvinyl chloride; 10 parts of triethanolamine, 4 parts of polyethylene glycol and 2 parts of cetanol sodium sulfate; 45 parts of dimethylformamide; 10 parts of hydroxypropyl methylcellulose; 8 parts of polymethyl methacrylate and 2 parts of dibutyl phthalate.
Example 2
The embodiment provides a large-flux reinforced ultrafiltration membrane which is composed of the following components in parts by weight: 40 parts of dopamine modified polyvinyl chloride; 15 parts of triethanolamine; 50 parts of dimethylacetamide; 15 parts of polyethylene glycol 300; and 12 parts of polysulfone.
Example 3
The embodiment provides a large-flux reinforced ultrafiltration membrane which is composed of the following components in parts by weight: 35 parts of dopamine modified polyvinyl chloride; 10 parts of triethanolamine, 4 parts of polyethylene glycol and 4 parts of cellulose acetate; 50 parts of dimethylformamide; 10 parts of hydroxypropyl methylcellulose and 5 parts of talcum powder; 8 parts of polymethyl methacrylate, 5 parts of polyethylene and 2 parts of dioctyl phthalate.
Example 4
The embodiment provides a large-flux reinforced ultrafiltration membrane which is composed of the following components in parts by weight: 30 parts of dopamine modified polyvinyl chloride; 16 parts of triethanolamine and 4 parts of triethanolamine oleate; 50 parts of dimethylacetamide; 10 parts of hydroxypropyl methylcellulose and 10 parts of talcum powder; and 5 parts of polystyrene.
Example 5
The embodiment provides a large-flux reinforced ultrafiltration membrane which is composed of the following components in parts by weight: 35 parts of dopamine modified polyvinyl chloride; 12 parts of triethanolamine and 5 parts of polysorbate; 40 parts of dimethylformamide; 10 parts of polyethylene glycol 600; 5 parts of polysulfone and 5 parts of polypropylene.
Example 6
The embodiment provides a large-flux reinforced ultrafiltration membrane which is composed of the following components in parts by weight: 40 parts of dopamine modified polyvinyl chloride; 10 parts of triethanolamine, 4 parts of propylene oxide-epoxy hexane copolymer and 4 parts of polyethylene glycol; 50 parts of dimethylformamide; 6 parts of hydroxypropyl methylcellulose and 4 parts of wood powder; 13 parts of polymethyl methacrylate and 2 parts of diisodecyl phthalate.
Example 7
The embodiment provides a large-flux reinforced ultrafiltration membrane which is composed of the following components in parts by weight: 35 parts of dopamine modified polyvinyl chloride; 10 parts of triethanolamine, 3 parts of dioctyl sodium sulfosuccinate and 5 parts of sodium lauryl sulfate; 45 parts of dimethylformamide; 6 parts of hydroxypropyl methylcellulose, 4 parts of wood powder and 2 parts of polyethylene glycol 600; 6 parts of polymethyl methacrylate and 4 parts of diisodecyl phthalate.
The preparation methods of the large-flux reinforced ultrafiltration membranes of the embodiments 1 to 7 are as follows, and specifically include the following steps:
s1, adding the dopamine modified polyvinyl chloride, the solvent, the hydrophilic agent, the pore-forming agent and the auxiliary agent into a stirring kettle respectively according to the proportion, stirring and mixing for 24 hours, controlling the temperature at 90-95 ℃ and the stirring speed at 100HZ, and obtaining a casting solution;
s2, conveying the stirred casting film liquid to a reaction kettle through a conveying pump for vacuum foaming for 12 hours;
s3, after defoaming, inputting the casting solution into a spinneret plate of a spinning machine through a metering pump, mixing the casting solution with pure water core solution, and then feeding the mixture into a coagulating bath for reaction, wherein the surface of the casting solution and the surface of the hollow fiber are coagulated and occluded after entering the water surface of the coagulating bath to generate a core liquid film;
s4, stretching the core liquid film through a wire winding wheel and bringing the core liquid film into a washing tank for collection and cutting;
s5, after the collection is finished, the core liquid film is immersed in 10-50% glycerol aqueous solution for 5-8 h and then dried.
Wherein: the preparation method of the dopamine modified polyvinyl chloride specifically comprises the following steps:
s1.1, dissolving Tris (hydroxymethyl) aminomethane in distilled water, and adjusting the pH to 8.5 by using hydrochloric acid to obtain a Tris-HCl buffer solution;
s1.2, rapidly adding polyvinyl chloride powder and ethanol or isopropanol or glycerol into the Tris-HCl buffer solution obtained in the step 1.1 under the condition of continuously magnetically stirring at room temperature;
s1.3, magnetically stirring the mixed solution obtained in the step S1.2 at 25 ℃ for 6-24 hours;
s1.4, carrying out suction filtration on the product obtained in the step S1.3, then washing with deionized water, centrifuging for 3 times, and placing the obtained product in a vacuum drier at 40 ℃ to dry to constant weight to obtain the dopamine modified polyvinyl chloride.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (5)
1. The large-flux reinforced ultrafiltration membrane is characterized by comprising the following components in parts by weight: 30-40 parts of dopamine modified polyvinyl chloride, 10-20 parts of hydrophilic agent, 40-50 parts of polar solvent, 10-20 parts of pore-forming agent and 5-15 parts of auxiliary agent;
the hydrophilic agent comprises triethanolamine, polyethylene glycol, polysorbate, cellulose acetate, propylene oxide-epoxy hexane copolymer, triethanolamine oleate, dioctyl sodium sulfosuccinate, sodium lauryl sulfate and cetanol sodium sulfate, wherein the mass of the triethanolamine in the hydrophilic agent is more than 50%;
the preparation method of the dopamine modified polyvinyl chloride specifically comprises the following steps:
s1.1, dissolving Tris (hydroxymethyl) aminomethane in distilled water, and adjusting the pH to 8.5 by using hydrochloric acid to obtain a Tris-HCl buffer solution;
s1.2, rapidly adding polyvinyl chloride powder and ethanol or isopropanol or glycerol into the Tris-HCl buffer solution obtained in the step 1.1 under the condition of continuously magnetically stirring at room temperature;
s1.3, magnetically stirring the mixed solution obtained in the step S1.2 at 25 ℃ for 6-24 hours;
s1.4, carrying out suction filtration on the product obtained in the step S1.3, then washing with deionized water, centrifuging for 3 times, and placing the obtained product in a vacuum drier at 40 ℃ to dry to constant weight to obtain the dopamine modified polyvinyl chloride.
2. The large flux reinforced ultrafiltration membrane of claim 1, wherein the polar solvent is dimethylformamide or dimethylacetamide.
3. The large-flux reinforced ultrafiltration membrane according to claim 1, wherein the pore-forming agent is one or more of hypromellose, talc, wood flour, polyethylene glycol 300, and polyethylene glycol 600.
4. The large flux reinforced ultrafiltration membrane of claim 1, wherein the auxiliary agent is one or more of polymethylmethacrylate, polysulfone, polypropylene, polyethylene, polystyrene, dibutyl phthalate, diisodecyl phthalate, dioctyl phthalate.
5. The preparation method of the large-flux reinforced ultrafiltration membrane according to claim 1, which is characterized by comprising the following steps:
s1, adding the dopamine modified polyvinyl chloride, the solvent, the hydrophilic agent, the pore-forming agent and the auxiliary agent into a stirring kettle respectively according to the proportion, stirring and mixing for 24 hours, controlling the temperature at 90-95 ℃ and the stirring speed at 100HZ, and obtaining a casting solution;
s2, conveying the stirred casting film liquid to a reaction kettle through a conveying pump for vacuum foaming for 12 hours;
s3, after defoaming, inputting the casting solution into a spinneret plate of a spinning machine through a metering pump, mixing the casting solution with pure water core solution, and then feeding the mixture into a coagulating bath for reaction, wherein the surface of the casting solution and the surface of the hollow fiber are coagulated and occluded after entering the water surface of the coagulating bath to generate a core liquid film;
s4, stretching the core liquid film through a wire winding wheel and bringing the core liquid film into a washing tank for collection and cutting;
s5, after the collection is finished, the core liquid film is immersed in 10-50% glycerol aqueous solution for 5-8 h and then dried.
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| WO2012047282A2 (en) * | 2010-09-30 | 2012-04-12 | Porifera Inc. | Thin film composite membranes for forward osmosis, and their preparation methods |
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| CN107149881A (en) * | 2016-03-02 | 2017-09-12 | 天津工业大学 | A kind of dopamine modifying polymer film and preparation method thereof |
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| CN101362055A (en) * | 2008-09-26 | 2009-02-11 | 复旦大学 | Preparation method of positively charged hyperfiltration membrane and products thereof |
| CN104226123A (en) * | 2014-09-04 | 2014-12-24 | 北京碧水源膜科技有限公司 | Preparation method of high-flux and anti-pollution reverse osmosis membrane and application of membrane |
| CN105948327A (en) * | 2016-06-26 | 2016-09-21 | 福建碧蓝环保股份公司 | Wastewater zero discharging treatment integrated equipment |
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| CN101920171A (en) * | 2010-08-25 | 2010-12-22 | 茅忠海 | Polrvinyl chloride hollow fibre ultrafiltration membrane preparation method |
| WO2012047282A2 (en) * | 2010-09-30 | 2012-04-12 | Porifera Inc. | Thin film composite membranes for forward osmosis, and their preparation methods |
| CN105492109A (en) * | 2013-10-04 | 2016-04-13 | Lg电子株式会社 | Surface-modified separation membrane and method for modifying surface of separation membrane |
| CN107149881A (en) * | 2016-03-02 | 2017-09-12 | 天津工业大学 | A kind of dopamine modifying polymer film and preparation method thereof |
| CN108246128A (en) * | 2018-02-07 | 2018-07-06 | 中国石油大学(华东) | A kind of loose reverse osmosis membrane of fatty polyamide and its preparation method and application |
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